Method of crystallization.



No. 780,448. PATENTBD JAN. 17, l1905.

V. SGHTZE. MBTHQD 0F GRYSTALLIZATION.

APPLIOATION FILED 16.53.18,'1904.

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No. 780,448.A

atented January 1'7, 1905.

PATENT OFFICE.

VICTOR soIITzE, oE RIGA, EUssIA.

N IETHOD OF CRYSTALLIZATION.

SPECIFICATION forming part of vLetters Patent No. 780,448, dated. January 17, 1905. i

' Application Jfiled March 18, 1904. Serial No. 198,831.

To all whom it Inwy concern.-

Beit known that I, VICTOR ScHTzE, a subject of the Czar of Russia, residing at Riga, Russia, have'invented certain new and useful Improvements in Methods of Crystallization; and I do hereby declare vthe following to bea full, clear, and exact descriptionof the inven-l In the accompanying drawings, which illustrate an apparatus for carrying out my invention, Figure 1 is a perspective view thereof. Fig. 2 is a longitudinal vertical section thereof. Fig. 3 is a longitudinal horizontal section thereof., Fig. 4t is an end view thereof, and Fig. 5 is a cross-section of the-same.

It is well known that crystallization takes is kept in movement.

am familiar labor under the diliiculty that perfect crystals can be obtained-only from solutions concentrated at a low temperature, never over 106O Fahrenheit,- while in case of wholesale manufacturing it is desirable to Work withsolutions concentrated at the highest possible temperature. If a solution which is concentrated at 2120 Fahrenheit until it becomes saturated is allowed to pass through an open vessel, the-matter vin solution will as the liquor becomes cooler b e deposited in an uncrystallized powdery form, which will not increase in size, whereas if perfect crystals-were formed, no matter how small, they would gradually increase in size. regular well-finished crystals in the case mentioned takes place only toward the end of the apparatus after theliquor has become con'- siderably cooler and much less concentrated,

and in an apparatus such as mentioned' it is impracticable to obtain regular well-finished crystals except toward the very end thereof.

The salts will first be deposited in the forml of powder, later on in conglomerate lumps cleaning the apparatus.

The separation of only partially crystallized and containing much mother-liquor. My inventionv is designed to doaway with these diiiiculties and to obtain regular well-.finished crystals from a satura-ted solution concentrated at a high heat, and is especially adapted for wholesale manufacturing. Y

To carry out my method perfectly, it is necessary that the concentrated solution should be cooled slowly and evenly at the same time, the result being that the small crystals deposited where the solution is hottest will gradually increase in size and the crystallization be perfected.

In the accompanying apparatus for carrying out my method, B represents an elliptical vessel into which the boiling saturated solution is delivered through the opening T and after depositing the salts -held thereby in the form of crystals passes out through the trough E. The vessel B is surrounded by a similarlyshaped larger vessel C, provided with an inlet-pipe K for the entrance of the cooling lliquid and a discharge M. The pipe K is vforked,` and in one of the forks, which supplies hot water to the apparatus. a stop-cock R is provided,'and in the other fork, which supplies cold water to the apparatus, a stopcock N is provided.

O represents openings ,which extend through both-of the vessels for the purpose of observing the progress of the crystallization and for i Ordinarily these, openings are closed by the covers D.

In carrying out my improved method the stop-cock R is opened and the space between irthe vessels B and C is filled with hot' Water having a temperature about 2120 Fahrenheitk until the liquid which passes out the pipe M shows atemperature a few degrees lower than that of the salt solution which comes in `through the opening T. vThe stop-cock R is then closed and the stop-cock N partially opened, allowing a veryslow iow. of c'old water through the pipe K into the space between the vessels B and C. The flow of water vthrough the apparatus is so regulated that when it passes out from the tube M it is a few degrees lower in temperature than the solution entering through the opening T. The

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solution Jfrom which the `crystals are to be eX- tracted is then allowed to ilow slowly through the opening T. Being a little warmer than the side of the vessel where it first strikes, this solution immediately begins to deposit small but fully-iinished crystals on the bottom of thevessel B just below the opening T. The solution as it passes through the vessel B becomes less and less concentrated and comes in contact successively with colder and colder portions of the vessel B, depositing more and more crystals, which crystals gradually grow in size as more and more of the solution flows over them, until inally the mother-liquor passes out of the trough E, having deposited a very large percentage of the salts therein dissolved. By regulating the temperature of the cooling liquid, which is done by regulating the How thereof, the amount of salts which the motherliquor still contains as it passes out of the apparatus can be regulated to a nicety. Furthermore, by this method it is possible to separate Jfrom each other diiferent salts contained in the same liquid. For example, supposing we have a solution saturated at 2120 Fahrenheit and containing equal parts of sulfate of copper and sulfate of iron, it is easy to find out after drawing4 up the curves of solubility of these salts what temperature of the cooling liquid is necessary in order to prevent one of said salts from being crystallized and practically crystallizing the whole or a large part of the other salt.

By my method the vessel B becomes gradually more and more illed up with well-finished crystals, which after having obtained the desired size pass out through the trough E, to-

gether with the mother-'liquoigwhichl of course has that degree of concentration which is determined by the temperature of the apparatus at the outlet end. The crystals thus obtained are placed on sieves, and after the motherliquor has drained off they are washed with a Very small quantity of water and then passed into a centrifugal machine and dried, making` them ready for commercial use.

Having thus described my invention, what I claim as new, and desire to secure by Letters Patent, is-

l. The method of obtaining crystals, which consists in causing a hot concentrated solution to pass slowly along, and periodically subjecting said solution in its passage to successivelyincreasing degrees of cold, substantially as described.

2. The method of obtaining crystals` which consists in causing a hot concentrated solution to pass slowly along and to be subjected in its passage to the action of a coolingl liquid slightly cooler than itself at the begi nning o1 said passage and gradually becoming colder, substantially as described.

3. The method of obtaining cr 'stals, which consists in causing a hot concentrated solution -to pass slowly through a vessel surrounded by a jacket containing coolingliquid,and regulating the supply of said cooling liquid so that the temperature thereof shall be slightly below that of the solution where it enters the ,vessel and gradually lessen in temperature up to the point where the cooling liquid enters the jacket, substantially as described.

In testimony whereof l aiiix my signature in presence of two witnesses.

VICTOR SCHTZE.

Vitnesses:

CoNsTANTIN PYGHLAU, ARTHUR BULLA. 

